溶剂吸收气相色谱-质谱法测定蔬菜与水果中二硫代氨基甲酸盐(酯)类农药残留  

Determination of dithiocarbamate residues in vegetables and fruits by gas chromatography-mass spectrometry

作　　者：张媛媛[1] 李延升[1] 韩晓鸥[1] 赵婉婧[1] 高岩[1] ZHANG Yuan-yuan;LI Yan-sheng;HAN Xiao-ou;ZHAO Wan-jing;GAO Yan(Center for Disease Control and Prevention of Liaoning Province,Shengyang 110005)

机构地区：[1]辽宁省疾病预防控制中心,沈阳110005

出　　处：《分析试验室》2019年第2期217-221,共5页Chinese Journal of Analysis Laboratory

摘　　要：在密闭加热的顶空瓶中,二硫代氨基甲酸盐(酯)类农药(DTCs)经HCl/SnCl_2溶液消化,反应生成CS_2气体被正己烷吸收,形成CS_2的正己烷溶液,采用气相色谱-质谱(GC-MS)检测CS_2的量,即代表DTCs农药的总残留量。通过蔬菜、水果样品中DTCs农药残留量的测定,对该方法进行了验证。用该方法测定时,CS_2在0. 02～10 mg/L范围内线性良好,相关系数r为0. 9999。福美双的转化率为93. 4%～97. 6%,精密度为1. 5%,符合要求。进行蔬菜、水果样品基质在3个添加水平的回收率实验,平均回收率范围为96. 4%～103. 8%,相对标准偏差为0. 39%～7. 4%。方法检出限为0. 005 mg/kg。In airtight heating headspace bottle, to carbon disulfide gas by HCl/SnCl2 solution.the dithiocarbamate pesticides (DTCs)were digested The carbon disulfide were absorbed by hexane,which formed carbon disulfide in hexane solution,and then determined by gas chromatography-mass spectrometry (GC -MS)for further quantification of DTCs pesticide residues.The method was validated by the determination of DTCs pesticide residues in vegetable and fruit samples.With this method,carbon disulfide had good linearity in the range of 0.02 -10 mg/L (r >0.9999 ).The conversion rates of thiram were within 93.4%-97.6%,and the relative standard deviations were 1.5%.The average recoveries at three adding levels in vegetables and fruits matrix were 96.4%- 103.8%and the relative standard deviations were 0.39%-7.4%.The limit of detection was 0.005 mg/kg.

关 键 词：二硫代氨基甲酸盐(酯)类农药 CS2 气相色谱-质谱 溶剂吸收法 蔬菜 水果 

分 类 号：TQ450.7[化学工程—农药化工]